Method of filling a container by vacuum and then placing the container under pressure



Jan. 10, 1950 A. J. RITCHIE 2,494,454

METHOD OF FILLING A CONTAINER BY VACUUM AND THEN PLACING THE CONTAINERUNDER PRESSURE Filed Aug. 10, 1944 FIG.E

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ALEXANDER J. RITCHIE ATTORNEYS Patented Jan. 10, 1950 unrreo srres.

Alexander J. Ritchie, Bayonne, N. 3., assignor to vElectric BoatCompany, Bayonne, N. J a corporation oi New Jersey Application August10, 1944, Serial No. 548,93!

2 Claims. (CL 226-116) This invention relates to synthetic smoke or fog,and has for its object the provision of an improved method of fillingcontainers with .smoke compositions comprising titanium tetrachloride asthe principal component and charging the container with apressure-creating medium. The invention is especially concerned with thefilling of containers with smoke compositions comprising titaniumtetrachloride. phosphorus and carbon bisulfide as the smokeformingmaterials, and carbon dioxide under pressure as the pressure medium.Smoke compositions of the character described in my copendingapplication Serial No. 471,079, filed January 1, 1943, now Patent No.2,407,384, of September 10, 1946,'may advantageously be charged intocontainers and placed under a suitable working pressure by the method ofthis invention. The invention is directed to the filling of -themetallic container (usually steel cylinders with closed ends) in whichthe composition is kept until discharged in creating a smoke. Theinvention also includes improvements in applying and using valves inconnection with ,such containers during the filling thereof with thecomposition and carbon dioxide.

I have discovered a method of filling containers with the components ofa smoke composition that results in greater emciency of time, materialand energy and which minimizes contamination of the composition. Thecomponents of the smoke composition react with and are impaired bywater. I have found that moistureladen air in the container isobjectionable. I have found that the removal of the air sufliciently toresult in a high vacuum effectively removes the moisture and that thevacuum may be used very advantageously in filling the container. I havefound that the smoke-producing composition comprising titaniumtetrachloride and a solution of phosphorus in carbon bisulfide may beintroduced into a substantially dry container by means of the vacuumwith a minimum of contamination and with the utmost safety to theworkmen.

In accordance with the method of my invention, I place the containerunder a high vacuum eliminating most of the air and its containedmoisture, and, by means of an appropriate valve apparatus, I suck theliquid smoke-producing composition into the container, either as amixand in an amount insumcient to fill the container leaving anappreciable space and a. residual vacuum of sufiicient sub-atmosphericpressure to suck in the solution of phosphorus and carbon bisulfide. Thecontainer is accordingly charged with the three components titaniumtetrachloride and the solution of phosphorus in carbon bisulfide bymeans ofthe suction of the vacuum. While I prefer to suck in thetitanium tetrachloride first, largely because of its greater volume, Imay reverse the order and suck in the solution of phosphorus in carbonbisulfide first,

and then admit the titanium tetrachloride. I may also suck them bothin-together. The container filled with the three components, as hereindescribed, is then charged with carbon dioxide under a high pressure,such as results from introducing liquid carbon dioxide.

I have found it -very advantageous to provide the container with aspecial valve which is used when the container is under a vacuum. Thisvalve is removed after the smoke-forming composition has been introducedinto the container. It is the usual practice to provide the chargedcontainer with a permanent valve that is usedto retain the compositionin the container for the discharge of the liquid in forming the smoke.In accordance with that preferred aspect of my invention in which Icharge the titanium tetrachloride and solution of phosphorus and carbonbisulflde in separately, I remove the special valve after charging thephosphorus and carbon bisulfide, thereby breaking the vacuum and thenattach the permanent valve. A source of carbon dioxide under highpressure such as a container of liquid carbon dioxide is connected tothe permanent valve and the desired quantity of carbon dioxide ischarged into the smoke composition in the container.

In the accompanying drawings:

Figs. 1 and 2 are diagrammatic illustrations,.

in side elevation, of arrangements of apparatus used in the invention.

of the cylinder l.

ture or as separate components, and then charge compressed carbondioxide into the container to subject the composition to -a highpressure. It is advantageous to keep the titanium tetrachloride and thesolution of phosphorus in carbon bisulfide separated until they arecharged into the container, and I, accordingly, use the vacuum to suckthe components in separately. I prefer to suck the titaniumtetrachloride in first In carrying out a method of my invention in thefilling of steel cylinders, the preliminary step is to remove anymoisture adhering to the inside This may be done bymeans of a blast ofair, preferably dry, warm or hot air. Those cylinders which have athreaded connection, or the like, for the attachment of the permanent ordischarge valve are provided with a temporary or filling valve 2. Thefilling valve 2 is connected to a vacuum pump 3, and, when a vacuum ofaround 28 inches of mercury is reached, the valveis closed anddisconnected from the vacuum pump by the coupling 6. The removal of airin creating the vacuum eifectively diminishes the gaseous water in thecontainer. A pipe 5 leading to a body of liquid titanium tetrachloridein the container 6 (under a pressure cedure is to place the container ona scales l and let the titanium tetrachloride be sucked in until thedesired weight has been reached. The introduction of titaniumtetrachloride reduces the amount of vacuum and I, accordingly, shutvalve 2 to interrupt the How at a point where .there is an appreciablevacuum left, sumcient at least, to suck in the carbon bisulfide andphosphorus solution and leave room for charging the carbon dioxide. Thepipe leading to the source of titanium tetrachloride is removed from thetitanium tetrachloride container 6 and inserted into the carbonbisulfide and phosphorous solution in container [2, as shown in brokenlines. 01 course, the pipe 5 may be disconnected from the valve andanother pipe connected for receiving the solution of phosphorus andcarbon bisulfide. The valve 2 is again opened and the desired quantityof the carbon bisulfide and phosphorous solution is sucked into thecontainer I. The tank is agitated to mix the titanium tetrachloride,carbon bisulfide and phosphorous solution together and facilitate theirintersolution. The pipe 5 and filling valve 2 are now removed, and, ofcourse, the vacuum is broken and the unfilled space in the tank is underatmospheric pressure. The permanent or discharge valve i5 (Fig. 2) isnow securely attached to the container and a pipe I6 is attached to thevalve leading to a source of carbon dioxide under a high pressure,advantageously a container ll of liquid carbon dioxide. The valve isopened and the carbon dioxide is run in until the desired pressure isattained. Ordinarily, carbon dioxide n an amount equal to about 5% ofthe weight of titanium tetrachloride is suiilcient for the purpose. Theamount of carbon dioxide is not critical, and more or less may be usedas conditions dictate. For normal conditions, a suificent amount ofcarbon dioxide should be charged into the container to provide apressure of around 150 to 180 pounds per square inch at roomtemperature.

In order to reduce the fire hazard in the handling of thephosphorous-carbon-bisulfide solution, I add carbon tetrachloride to thesolution before mixing the solution with the titanium tetrachloride.From about A to 1 part (by weight) of carbon tetrachloride per part ofcarbon bisuliide is sufilcient for the purpose.

The following is an example of a typical operation for filling a steelcontainer having a capacity of about 278 pounds of water. The driedcontainer I with the filling valve 2 attached is placed under ,a vacuumof about 28 inches of mercury, and then the valve is connected to pipe Iwhich is inserted into tank 6 of liquid titanium tetrachloride. Thevalve is opened and 308 pounds of titanium tetrachloride (sp. gr. 1.74)are run into the container l. The valve is closed and the pipe isremoved from the titanium tetrachloride and dipped into vessel I2 havinga solution comprising 2 pounds of carbon bisulfide, 8 ounces ofphosphorus and 1.5 pounds of carbon tetrachloride. The valve 2 is openedand this solution is sucked into the container. The container isagitated to facilitate intermixing and solution of the materials. Thepipe 5 and valve 2 are disconnected from the container I. exposing thecontents to atmospheric pressure, and the permanent valve II is securelyattached by means oi threads to the container. The threaded dischargeend of the valve is connected to pipe ll leading to tank 11 of liquidcarbon dioxide. The valve is opened, I! pounds of carbon dioxide arecharged into the container, and the valve 15 is closed tightly. The pipeis removed, a protecting cap not shown is placed over the threadeddischarge end II, and the charged container is ready for shipment to thearmed forces. It is only necessary to attach a suitable nozzle to thethreaded discharge end of the valve and open the valve to discharge thesmoke composition and make the smoke.

I claim: j

1. The method of charging a container with a smoke compositioncomprising titanium tetrachloride, carbon bisulfide and phosphorus whichcomprises placing the container in a substantially dry condition under avacuum, using the vacuum to suck titanium tetrachloride into thecontainer, stopping the flow of titanium tetrachloride into thecontainer leaving an appreciable space and a partial vacuum therein,then using the remaining vacuum to suck a solution of phosphorus incarbon bisulflde into the container, and then charging liquid carbondioxide into the container.

2. The method of charging a container with a smoke compositioncomprising titanium tetrachloride, carbon bisulfide and phosphorus whichcomprises attaching to the container a filling valve, placing thecontainer in a substantially dry condition under a vacuum. attaching aduct leading to a source of titanium tetrachloride to the valve andopening the valve to suck the charge of titanium tetrachloride into thecontainer, closing the valve before the container is filled withtitanium tetrachloride whereby an appreciable space and a partial vacuumremain in the container, connecting the valve by a duct to a solution ofphosphorus in carbon bisulfide. removing the filling valve and attachinga discharge valve to the container, connecting the discharge valve to asource-oi carbon dioxide under pressure and charging the carbon dioxideinto the container, and closing the discharge valve and disconnecting itfrom the source of carbon dioxide.

' AIEXANDER J. RITCHIE.

REFERENCES crrsn The following references are of record in the file ofthis patent:

UNITED STATES PATENTS Number Name Date 421,076 Holgate Feb. 11, 18901,010,869 Davidson Dec. 5, 1911 1,303,749 Wilkinson May 13, 19192,025,141 Werder Dec. 24, 1935 2,059,455 Hoar Nov. 3, 1936 2,126,532Cate Aug. 9, 1936 2,126,563 Lee Aug. 9, 1938 2,146,072 Howard Feb. 7,1939 FOREIGN PATENTS Number Country Date 492,506 Great Britain Sept. 21,1938

